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By O. J. Huber, P. D. Frost, H. A. Robinson

URANIUM is a (ß-stabilizing, eutectoid-forming element when alloyed with titanium. Udy and Boulger1 have reported that an alloy of 48.6 pet uranium in titanium retains ß-phase when quenched from the ß-region, while compositions of approximately 30 pet uranium transform to martensite during such quenching. Since the eutectoid reaction is rather sluggish, titanium-uranium alloys should be capable of being strengthened by the ß — a trans-

Jan 1, 1959

By J. F. Radavich

Many heats of steel of low carbon value have been known to produce brittle pieces of steel. The brittleness is believed to be due to the impurities located within the grain boundaries. Such brittle steels have been examined with an optical microscope to ascertain the nature and the amount of the impurities present at the grain boundaries. Due to the relatively low resolving power of the optical microscope, the impurities are not visible in fine detail. The writer obtained some sheet steel and proceeded to determine the location of the impurities and to show the application of the electron microscope to the study of grain boundaries. One sample was known to be capable of becoming embrittled, whereas another sample was believed to be much less susceptible to embrittlement. Treatment of Specimens The specimens were embrittled by annealing above the A3 point under mildly oxidizing conditions. One piece of ingot iron could not withstand a 90" bend, whereas another piece of ingot iron was not affected and could withstand a 90" bend. The brittle piece was then annealed at a high temperature in a hydrogen atmosphere. The annealed ingot iron was termed cured and could withstand a 90" bend very easily. The three specimens examined will be designated as brittle, good. and cured in the discussion that follows. Procedure The sizes of the specimens were as follows: one piece of brittle ingot iron-3/8 by 35 in.; one piece of good ingot iron-96 by 1/8 in.; one piece of cured ingot iron-36 by 54 in. The specimens were too small to be polished by hand and therefore were mounted in bakelite. The polishing procedure was carried out in the conventional manner with the use of 1/0 through 3/0 papers, and the final polish was done with alumina on a billiard cloth. The specimens were then etched in a 4 pct solution of picral in alcohol, and then they were examined through an optical microscope. An area was chosen that showed distinct grain boundaries, and an effort was made to keep near this area when pulling the replicas REPLICA TECHNIQIJE The replica technique used in the preparation of the replicas for examination under the electron microscope is described in Electron Metallography.' It consists essentially of the following steps: 1. Obtaining a suitably etched specimen. 2. Applying a swab of ethylene di-chloride on the surface. 3. Applying a formvar solution on the surface. 4. Placing a screen on any desired spot. 5. Breathing on the fornivar layer. 6. Applying scotch tape on the screen and film. 7. Pulling the film and the screen up with the Scotch tape. 8. Separating the screen from the Scotch tape. This replica technique is very similar to the one described by Harker and Shaefer. However, with the added step, the percentage of replicas removed is very much higher regardless of the length of the time from the etching of the specimen to the actual pulling of the replica. The replicas were then shadow cast with manganese at a filament height to replica distance ratio of 1 1/2:7. This produced a very high contrast replica for use in the electron microscope. One of the dificulties encountered with this study was the restricted area of the specimen. The width of the specimens was the same as that of the 200 mesh nickel supporting screen. In order to increase the effective area, the screens were cut down as shown in Fig 1. The arrow indicates the direction in which the replica was pulled. This operation made it possible to obtain a large percentage of good replicas. Fig 3 shows an electron micrograph of a brittle piece of ingot iron and a grain boundary that was polished mechanically. The surface is very rough probably due to the incomplete removal of the flowed layer by the picral etchant. The grain boundary does show evidence of impurities. It was decided to electropolish the specimens to obtain a much smoother surface than the one obtained by mechanical polishing. ELECTROPOLISHING The specimens were cut in half to expose the metal on the back side. The exposed metal had sufficient area to make good electrical contact and electropolishing was carried out easily. The conditions for electropolishing were 0.9 amp, 35 volts, and 25 sec. in an electrolyte composed of 850 cc of ethyl alcohol, 100 cc distilled water, and 50 cc of perchloric acid. The polished specimens were then etched in the 4 pct picral solution for a shorter time than was necessary for

Jan 1, 1950

By I. R. Kramer

Studies of the effect of size of the specimen on the change of slopes of Stages I and 11 by surface removal showed that the change of Stage I was independent of size with respect to the polishing rate; however, the change in the slope of Stage 11 with polishing rate increased directly in proportion to the surface area. The removal of the surface during the test affected the plastic deformation characteristics of gold, aluminum, and zinc single crystals and polycrystalline aluminum. The apparent activation energy of aluminum was found to be decreased markedly by removing the surface during the deformation process. In previous papers1-3 it was shown that the surface played an important role in the plastic deformation of metals. By removing the surface layers of a crystal of aluminum by electrolytic polishing during tensile deformation, it was found that the slopes of Stages I, II, and III were decreased and the extents of Stages I and II were increased when the rate of metal removal was increased. By removing a sufficient amount of the surface layer after a specimen had been deformed into the Stage I region, upon reloading, the flow stress was the same as the original critical resolved shear stress and the extent of Stage I was the same as if the specimen had not been deformed previously. The slope of Stage I was decreased 50 pct and that of Stage 11 decreased 25 pct when the rate of metal removal was 50 X 10"5 ipm. These data show that in Stage I the work hardening is controlled almost entirely by the surface conditions, while in Stages 11 and III both surface conditions and internal obstacles to dislocation motion are important. It appears that during the egress of dislocations from the crystal, a fraction of them becomes stuck or trapped in the surface regions and a layer of a high dislocation concentration is formed. This layer would not only impede the motion of dislocations, but would provide a barrier against which dislocations may pile up. In this case, there will be a stress, opposite to that of the applied stress, imposed on the dislocation source and dislocations moving in the region beyond this layer. It has been found convenient to refer to this layer as a "debris" layer. The "debris" layer may be similar to the dislocation tangle observed by thin-film electron microscope techniques.4 Reported in this paper are the results of studies on the effects of removing the surface during plastic deformation on aluminum crystals of various sizes. The effects of the surface on the yield point behavior of gold and high-purity aluminum crystals as well as the creep behavior were also determined. The effects of surface removal on polycrystalline aluminum (1100-0 and 7075-T6) are also reported. EXPERIMENTAL PROCEDURE For those portions of the investigation involving creep and tensile specimens, single crystals, having a 3-in. gage length and a nominal 1/8-in. sq cross section, were prepared by a modified Bridgman technique using a multiple-cavity graphite mold. The single crystals were prepared from materials which had initial purities of 99.997, 99.999, 99.999, and 99.999 pct for Al, Cu, Zn, and Au, respectively. The aluminum specimens for the size effect studies were prepared through the use of a three-tier mold in which crystals having a cross section of 1/8, 1/4, and 1/2 in. were grown from a common seed. The mold design was arranged so that one 1/2-in. crystal, two 1/4-in. crystals, and four 1/8-in, crystals of the same orientation could be cast. With this technique, it was possible to obtain only one set of crystals with the same orientation. Because of this limitation, it was not possible to determine both the changes of extent and slope of the various stages since a large number of crystals of the same orientation would have been required. Instead, only the change of slope as a function of the rate of metal removal was studied by abruptly altering the current density of the electrolytic polishing bath at various strains within the regions of Stages I and 11. The experimental techniques used for the tensile studies were essentially the same as those used previously.1,3 The specimens were deformed in a 200-lb Instron tensile machine, usually at a rate of 10-5 sec-5. A methyl alcohol-nitric acid solution was used as the polishing bath for aluminum. The temperature was maintained constant within ±0.l°C by means of a water bath. The tensile machine was

Jan 1, 1963

Jan 1, 1940

By Read Winterburn

This discussion covers only one method of pressure drilling—that developed in the Kettleman Hills field. Thus it is probable that many departures from the procedure herein described would be advisable, and perhaps necessary, in using this method of drilling wells in other localities. Purpose of Pressure Drilling By the early part of 1936, formation pressures in the heavily produced north end of the Kettleman North Dome field had declined to range from 1000 to 1500 lb. per sq. in. This low pressure, combined with the depth of the wells (8000 to 9000 ft.) permitted water to be filtered out of the mud into the producing sands during drilling operations. The loss of water was indicated by loss of fluid from the suction tank while drilling, accompanied by an increase in mud weight. It was found that when water was added to the mud stream at such a rate as to keep the fluid level in the suction tank constant, the mud weight would not vary. This indicates that water only was forced into the sands. The rate of this loss at various wells ranged from 2 to 5 bbl. per hour. At some places complete loss of circulation occurred, and drilling mud to the extent of 200 to 1000 bbl. had to be pumped into the sands before returns were regained. It was believed that these conditions had already begun to harmfully affect production, and that such effect would become more pronounced as formation pressures continued to decline. Pressure drilling with oil was introduced because it eliminated the danger of loading the formations with mud and water. The method also afforded a convenient means of testing as drilling progressed, lessening the amount of formation testing, which had become necessary because of encroaching edge water.

Jan 1, 1938

By D. G. Westlake

The electrical resistance of a series of V-H alloys (0 to 3.5 at. pct H) has been measured over the temperature range G° to 360°. Interstitial impurities made contributions to the residual resistivity, but not the ideal resistivity. The contribution of hydrogen in solid solution is expressed by Ap = 1.12 microhm-cm per at. pct H; but the contribution of precipitated hydride was negligible. A portion of the so1vu.s for the V-H phase diagram is presented. The solubility limit is given by In N (at. pct H) = (5.828 i 0.009) - (2933 i 44)/RT. Comparison of critical temperatures joy hydride precipitation and published critical temperatures for hydrogen embrittlement suggests the two are related. ThiS study was initiated as part of an investigation of the mechanism by which small concentrations of hydrogen embrittle the hydride-forming metals at low temperatures. It has already been shown that, in the case of hcp zirconium, a reduction in ductility accompanies the strengthening resulting from precipitation of a finely dispersed hydride phase.''' Our attempts to detect a similar precipitation of a second phase at low temperatures in V-H alloys by transmission electron microscopy have been thwarted because we have been unable to prepare thin foils that are representative of the bulk material with respect to hydrogen concentrati~n.~'~ The present investigation establishes the solvus of the V-H system at subambient temperatures. Subsequently, we hope to be able to determine whether the embrittlement temperature is related to the critical temperature for precipitation of the hydride in a given V-H alloy. veleckis5 has proposed a partial phase diagram for the V-H system based on extrapolations of the pressure-composition relations he measured at higher temperatures. Kofstad and wallace' conducted a similar study of single-phase alloys but did not attempt to establish the phase diagram. Zanowick and wallace' and ~aeland' have studied a portion of the phase diagram by X-ray diffraction, but they investigated no alloys in the hydrogen concentration range 0 to 3 at. pct, the range of interest to us. EXPERIMENTAL PROCEDURE The vanadium was obtained from the Bureau of Mines, Boulder City, Nev., in the form of electrolytic crystals. The analyses supplied with them listed 230 ppm by weight metallic impurities, 20 ppm C, 100 ppm N, and 290 ppm 0. The crystals were electron-beam-melted into an ingot that was rolled to 0.64 mm. Strips, 60 mm long and 4.2 mm wide, were cut from the sheet, and both rolled surfaces were ground on wet 600-grit Sic paper to produce specimens 0.4 mm thick. They were wrapped in molybdenum foil, vacuum-encapsulated in quartz, and annealed 4 hr at 1273°K. The specimens were annealed in a dynamic vacuum of 2X lo-' Torr for 30 min at 1073°K for dehydrogenation, and charged with the desired quantity of hydrogen by allowing reaction with hydrogen gas at 1073°K for 2 hr and cooling at 100°K per hr. Purified hydrogen was obtained by thermal decomposition of UH3. Sixteen specimens were studied: two contained no hydrogen and the others had hydrogen concentrations between 0.5 and 3.5 at. pct (hydrogen analyses were done by vacuum extraction at 1073°K). Electrical resistances were measured by the four-terminal-resistor method on an apparatus similar to the one described by Horak.~ The specimen holder was designed so that both current and potential leads made spring-loaded mechanical contact with the specimen. The potential leads were 30 mm apart, and the current leads were 55 mm apart. The current was 0.10000 amp. We used the following baths for the indicated temperature ranges: liquid nitrogen, 77°K; Freon 12, 120" to 230°K; Freon 11, 230" to 290°K; and ethanol, 290" to 340°K. Temperatures lower than 77°K were achieved by allowing the specimen to warm up after removal from liquid helium. Temperatures above 77°K were measured by a calibrated copper-constantan thermocouple (soldered to the specimen holder) and below 77°K by a calibrated carbon resistor. The temperature of the bath changed less than 0.l0K between duplicate measurements of the resistance. RESULTS AND DISCUSSION Typical plots of resistivity p vs temperature T are shown in Fig. 1. In the interest of clarity, only five curves are presented and the data points have been

Jan 1, 1968

By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.' Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-' and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964

THE 144th* meeting of the American Institute of Mining and Metallurgical Engineers was held in New York, Feb. 18 to 21, 1935. It consisted of the annual business meeting, 45 technical sessions at which 216 papers were presented (approximately the same number of sessions and papers as at the previous annual meeting), two sessions of the Board of Directors, three meetings of Section delegates, two formal lectures and two addresses, luncheon Monday, Tuesday and Wednesday for members and guests, six group dinners and eight group luncheons, ten committee meetings, the annual reception and dinner dance, an informal dance, a smoker-dinner and the annual meeting of the Woman's Auxiliary. Attendance was generally greater than for the two preceding meetings; the statistics follow (figures are in the order 1935-1934-1933); total registration, 1609-1534-1475; dinner dance, 577-543-426; dinner-smoker, 490-425-394; informal dance, 279-295-250; women's registration, 179-160-133; general luncheons, 1132-1034-734. The Coal Division held two general sessions on Monday and a symposium on coal-mine ventilation on Tuesday morning. The Committee on Bituminous Planning, Edward Steidle, chairman, presented a report at the Monday morning session. C. B. Huntress, President of Appalachian Coals, Inc., was the principal speaker at the luncheon on Monday, at which Eli T. Conner, Chairman of the Division, presided. Mr. Huntress was preceded by Howard N. Eavenson, President of the Institute, who spoke briefly. The Sectional Committee on Classification of Coal met Wednesday afternoon. A feature of the meeting concerning three Divisions-Iron and Steel, Institute of Metals, Petroleum-was the symposium on Use of Metals in the Petroleum Industry, Thursday morning and afternoon. Five of the papers presented at this symposium have been published in METALS TECHNOLOGY'. Another feature, of general interest, was the Tuesday morning session in the Auditorium, devoted to Federal Government and Mineral Industries. Dr. C. K. Leith delivered the principal address, on "A, Mineral Policy for the United. States." . The Institute of Metals Division held technical sessions Tuesday afternoon and Wednesday. morning and afternoon and on Thursday

Jan 1, 1936

By J. T. Peters, N. Schapiro, R. J. Gray

Petrographic studies of coal have resulted in a better understanding of the origin and composition of coal and have added to the knowledge of how and why coals differ in their response to various prepamtion and utilization processes. Petrographic methods can now be used in scientific economic exploitation of coals. Because the United States Steel Corp. is one of the largest consumers of coal and coke, there is a continuing interest in the corporation in perfecting a better understanding of coal so that it can be utilized more effectively. Coal is a heterogeneous substance composed principally of plant material that has been altered by a complex geochemical process to form rock. The science of coal is anthracology. The ultimate aim of anthracology is determining the relationships and differences among coals. The fundamental aim is finding out why coals differ. The practical application is determining how the differences in coals affect their utilization properties. Coal, like other sedimentary rocks, consists of more than one material. Fig. 1, a photograph of a natural fracture and a polished surface of a lump of coal, displays heterogeneity in terms of the banded ingredients present. The earliest attempts to describe coal were based on its hardness and appearance. ' Thus, coal has been described as hard or soft, bright or dull, and banded or nonbanded. The variations in the hardness and physical appearance of the coal reflect differences in materials that constitute the coal. The banded nature, lustre, and texture depend upon the relative proportions of the various constituent materials. Even the earliest petrographic investigations of coal produced evidence of of the heterogeneity of the coal substance and shoul have destroyed the concept of the unit coal molecule. Coals (Fig. 2) that appear the same frequently consist of different microscopic materials and may behave differently during mining, pulverization, washing, or coking. In Fig. 3, the upper photograph shows a bright at-trital medium-volatile coal, and the micrograph at the right shows some of the materials that constitute the coal. The lower photograph shows a bright attrital low-volatile coal and the corresponding micrograph shows material of similar origin to those from the medium-volatile coal. Any petrographic description of a coal that has meaning in terms of its utilization begins with a microscopic examination. Numerous attempts have been made to describe coal on the basis of the materials that constitute the coal.2*3 Initial petrographic studies were directed towards the question of the origin of coals without any true basis for studying the metamorphic changes in the

Jan 1, 1962

By H. H. Uhlig

A study of passivity in chromium-iron alloys holds considerable interest, both because of the present-clay practical importance of the stainless steels, and because of the scientific importance attached to the mechanism of their corrosion resistance. Upon the discovery of the passive chromium-iron alloys in 1912, it seemed logical to attribute the observed phenomenal corrosion resistance to a thin, continuous, protective reaction product on the surface. The product was thought to be Cr2O3 or a similar oxide containing both chromium and iron. This mechanism seemed likely in view of Michael Faraday's conjecture that passive iron is not reactive in concentrated nitric acid because of an oxide on the metal surf ace. Since 1912, data have accumulated that permit a further exploration into the nature of passivity and provide a new approach to the problem. A summary of the facts lends considerable weight to a mechanism based not on physical protection of an oxide or similar compound, although such compounds may be present on the surface, but to a change in tendency of surface metal atoms to react chemically. This change in reaction tendency is ascribed to chemisorbed films that effectively satisfy residual valence forces of the metal surface, but do not appreciably disturb the positions of metal atoms in the lattice. In other words, formation of a new lattice such as that of an oxide is not a necessary condition for this type of passivity. The decreased reaction tendency of the metal by reason of chemisorbed films can thereby account for low reaction rates of the stainless steels in many media, as well as a noble galvanic potential as is observed. Substances capable of adsorbing on the stainless steels, and hence accompanying the property of passivity, are typically oxygen, nitrites or chromates, but are not in any sense limited to these. Other elements and compounds can also chemisorb, and therefore may also play a major part in the mechanism of passivity in specific media. The mechanism of passivity based on chemisorption or activated adsorption begins with the interpretation Langmuir proposed for his experiments concerning adsorbed oxygen on tungsten.' He found that adsorbed oxygen was tightly bound, remaining on the tungsten surface above temperatures at which WO3 rapidly volatilizes. The oxygen in such a state did not readily react with hydrogen even at

Jan 1, 1949

UNIVERSITY OF ALABAMA University, Ala Mining and Metallurgical Society G T Bator UNIVERSITY OF ALASKA College, Alaska Mining Society Earl H Beistline-

Jan 1, 1952

The following figures (Nos. 1-4) and tables (Nos. 1 and 2) were inadvertently omitted from the chapter entitled "Optimum Open-Pit Mine Production Scheduling" by Thys B. Johnson, Section 4, pages 539-562. [ ]

Jan 1, 1969

By D. N. Stevens, D. N. Bloom, M. A. Klugman

This paper represents a portion of a larger study concerning dispersion of major, minor and trace elements in wall-rock about orebodies in part of the Colorado Mineral Belt. This phase of the work pertains to the Mg/Ca ratio variations in wall-rock adjacent to orebodies in two mines, one in the Horseshoe Mining District (Hilltop mine), and the other in the Alma Mining District (Phillips mine). The two districts lie adjacent to one another, the Horseshoe District on the south and the Alma District on the north, and are commonly referred to as one, the Alma-Horseshoe Mining District. The Alma-Horseshoe Mining District is located 80 miles southwest of Denver, Colo., (Fig. 1) in Park County, on the eastern slope of the Mosquito range. The area is typified by rugged relief with altitudes of from 10,500 to 14,000 ft. The Horseshoe District is separated from the Lead-ville Mining District by the crest of the Mosquito range, with the Leadville District to the west. The Alma-Horseshoe District has been considered as peripherial to the Leadville District, and has not received the detailed attention that the Leadville District has. These two mines were selected for this study because of their ease of access; the attitude of the workings and the drill holes to the known mineralization; the similarity of the mineralization; and because the mineralization occurs in carbonates in both mines but are of different ages. In the Hilltop mine mineralization is confined to the Leadville dolomite (Mis-issippian) and is principally lead with subordinate zinc and silver. In the Phillips mine the mineralization occurs in the Peerless dolomite and shale (Cambrian) and in the Manitou dolomite (Ordovician) and is principally zinc with subordinate lead, silver,

Jan 1, 1964

By J. G. Savins

Analytical procedures are described for optimizing the selection of a rheological model when it is desired to express the functional relationship between true shearrate and shearing stress in analytical form. The procedures are extended to two principal model categories — "Generalized Newtonian" and "Viscoplastic" models. Graphical examples are presented to illustrate the utility of certain characteristic deriuative functions in distinguishing between these categories and in determining how well a particular model reflects the flow behavior of rheologically anomalous materials in simple shearing flows. INTRODUCTION Modern drilling fluids and fracturing fluids, being chemically complex, are frequently non-Newtonian — a peculiarity which complicates the solution of problems such as designing flowline and process equipment, and predicting laminar-turbulent behavior, solid-suspending ability and cutting-transport efficiency. Therefore, techniques of data analysis which accurately characterize the behavior of rheologically complex materials are needed for the accurate formulation of solutions of these and similar problems. It is the purpose of this paper to describe the application of a sensitive method of rheological data analysis — the dual differentiation-integration method of optimizing the selection of the functional relation between shear rate and shearing stress — to a variety of materials of interest in drilling and production practices. BASIC CONCEPTS THE DIFFERENTIATION METHOD To a first approximation, the viscosity function for a non-Newtonian system can be expressed in a form analogous to Newton's law of viscosity by the following generalization2.3 between the stress On introducing the restrictions that the system is incompressible and the motion is rectilinear, then l = 0 and l3 = 0 ; and with the further restriction that the flow is slip-free, the viscosity (an invariant) is then determined solely by 12. With this approach one can set up a suite of integral equations relating observed kinematical and dynamical parameters for certain types of flow experiments involving simple shearing motion, e.g., flow in a cylindrical tube, flow between rotating concentric cylinders, and flow between fixed parallel surfaces of large aspect ratio. Taken in the order cited, these integral equations are as follows.

By J. C. Scully, G. Sanderson

The electrolytic formation of y hydride in thin foils of Ti-5Al-Z.5Sn alloy and four Ti-A1 binary alloys has been studied by electron microscopy and electron diffraction. Two orientation relationships have been found: THE adsorption of hydrogen by titanium alloys from aqueous solutions has been widely reported. This can occur, for example, in both alkaline' and acidic2 pickling baths, in chemical polishing374 and electro-polishing Solutions,3,4 during cathodic polarization5" and under certain corrosion conditions,7,8 Etching reagents may also produce visible precipitates, sometimes after an aging period.9 During an investigation into the stress corrosion susceptibility of a titanium alloys by thin foil electron microscopy many observations have been made of hydride precipitation which has been deliberately promoted by techniques that are described below. The characteristics of hydride precipitation are reported and the observed crystallographic orientation relationships are discussed with reference to distortion in the titanium lattice created by the presence of the hydride. EXPERIMENTAL TECHNIQUE One grade of commercial titanium and five alloys were examined. Their composition and hardness values are shown in Table I. All the materials were in the form of thin sheet, 0.05 to 0.065 cm thick, which had been annealed after cold rolling. Foils suitable for transmission electron microscopy were made in two ways: a) by chemical polishing; and b) by elec-tropolishing. The solution used for chemical polishing was a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. During this polishing specimens were manually moved up and down in the solution. The reaction was veFy rapid, specimens thinning to foil thickness (2000A) in 5 min. Since chemical polishing solutions tend not to cause hydride contamination if they are kept cool3 no attempt was made to prevent the solution from becoming hot during the thinning operation. Electropolishing was performed at -30° C with a mixture3 composed of 295 cu cm methyl alcohol, 175 cu cm n-butyl alcohol, and 30 cu cm perchloric acid with an applied voltage of 40 v after chemically thinning specimens to approximately 0.017 cm thickness in a cool solution of 44 pct HF, 40 vol H2O2, and water in the volumetric ratio 1:6:3. EXPERIMENTAL RESULTS 1) Ti-5A1-2.5Sn Alloy. The Ti-5A1-2.5Sn alloy was severely contaminated by hydrogen during the chemical polishing. Foils obtained in this way contained large amounts of the y hydride phase. A typical micrograph is shown in Fig. l. The laths were identified as the hydride phase by selected-area diffraction of a large number of foils examined in a tilting stage that could be turned through 40 deg. Using the lattice spac-ings of the alloy obtained by X-ray diffraction as a standard the a value of the hydride was determined fromo the electron diffraction patterns to be 4.38 to 4.40A. The accuracy of this figure is only about ±2 pct. Further evidence of the identification was obtained by vacuum annealing chemically polished foils of the alloy at 500°C. This resulted in the dissociation of the hydride with the production of dislocations and possibly vacancy loops as shown in Fig. 2. The hydride

Jan 1, 1968

Jan 1, 1944

By A. T. Aldred, K. M. Myles

The vapor pressure of chromium over solid V-Cr alloys has been measured by the torsion-effusion method in the temperature range 1450" to 1650°K. The chemical activities as well as the free energies, entropies, and enthalpies of formation of the alloys have hem computed from the vapor-pressure data. The activities of both chromium and vanadium exhibit fairly small negative deviations from Raoult's law over the entire composition range. The values of the excess entropies and the enthalpies of formation found at 1550°K are considered in terms of the changes in the clzaracteristic properties of vanadium and chromium that occur upon alloying. RECENT interest in the theory and properties of transition-metal alloys has shown the need for relevant thermodynamic data. The present investigation of the V-Cr system was undertaken as part of a more general study of thermodynamic properties of transition-metal alloys. The system was chosen because of the reported complete solid solubility of the components at all temperatures1 and because the difference in magnitude of the vapor pressures of vanadium and chromium allowed a simple effusion technique to be used. The torsion-effusion method was employed to minimize compositional changes in the alloys during the experiments. EXPERIMENTAL Equipment. The torsion-effusion apparatus, shown diagrammatic ally in Fig. 1, consists of a torsion system suspended inside a vertical vacuum chamber whose lower end is surrounded by a high-temperature vacuum furnace. An auxiliary optical lever and screen are used to determine the angle of rotation of the effusion cell. The torsion fiber is an annealed, high-purity, tungsten wire usually between 0.003 and 0.007 cm in diameter and about 43 cm long. The wire supports a concave mirror and a rigid tantalum connector tube. The effusion cell is fastened to the lower end of the connector tube by a dovetailed yoke and har- ness arrangement. The cells, which are 1.27 cm in diameter and 4.4 cm long, were made by electron-beam welding tantalum endcaps onto a 0.025-cm-wall tantalum tube. The two orifices, formed by drilling, have similar areas ranging from 0.011 to 0.031 sq cm. The noninductive sheath-type furnace consists of a single-phase tantalum heating element 6.35 cm in diameter, 15 cm high, and 0.013 cm thick; the element is completely surrounded by radiation shields in an evacuated chamber. The power system includes a 17-kva self-saturating saturable core reactor with an integral magnetic amplifier and a water-cooled, 15-kva, step-down power transformer with a multitap secondary. Temperatures are controlled to within ±1/2o at 1600°K by means of a unit that includes a reference voltage source, a dc electronic null detector, a current-adjusting proportional band relay, and the self - saturating reactor. At 1650°K the temperature variation within the cell, vertically and horizontally, is 3/4oK. Unwanted motions of the torsion system are damped by the movement of an aluminum vane, which is mounted on the connector tube, between the poles of an electromagnet. When not in use the magnet is withdrawn and rotated 90 deg to prevent its interaction with the rotation of the system. Measurements. The vapor pressure, p, is re-

Jan 1, 1964

By Guy R. Johnson

It is a common observation among those engaged in the ironbusiness, that the lower (i.e., the less graphitic) grades of pigiron show a rough face on the pig. As such irons are always low in silicon, the generally accepted belief is, that this rough face is due to the absence of silicon. Certain investigations, however, made by the writer on Embreville pig-iron, and extending over nearly a year's time, seem to indicate another cause, namely, the giving-off of included gases, particularly sulphurous oxide (SO2,). It is, of course, the tendency of such gases to rise through the iron, escaping into the air; and the more liquid the iron, and the longer it remains liquid, the greater the chance for such escape. The lower grades of iron, being always colder, tend to solidify early, and before the included gases can completely escape.

Jan 1, 1898

Map

Jan 1, 1944

By J. T. Burwell, J. Wulff

As is well known, the alloys of iron containing 18 ± per cent chromium, 8* per cent nickel and less than 1.2 per cent carbon exhibit the same allotropic modifications as iron. The face-centered cubic or gamma phase is stable at high temperatures and the body-centered cubic or alpha ferrite is presumably stable at room temperature. The transformation from the gamma phase to the alpha phase in alloys of the above composition (18-8 or stainless steel) is sluggish; even moderately rapid cooling permits the retention of the gamma phase. Cold-work, however, causes the transformation from gamma to alpha to occur at room temperatures. It is difficult, nevertheless, to induce complete transformation regardless of the method of cold-working. Since metallographic polishing is very effective in transforming the surface austenite to ferrite, as indicated by the magnetic studies of Buehl and Wulff,1 it was decided to investigate the phenomenon by electron diffraction methods. Apparatus The apparatus used (Fig. 1) was a hot-filament type employing movable slits, similar to that described by Germer.2 The sample-to-photographic plate distance was 69 cm. and the accelerating voltage 30 kv. Since electrons do not in general follow geometrical paths, it is necessary that either the electron source or the sample be movable in a plane normal to the beam. In this case the sample is fixed and the electron source is movable. The source is adjusted until the shadow of the sample appears in the brightest part of the beam as viewed on the fluorescent screen, then the slits composing the two pinholes are inoved into position one by one. The system is evacuated by means of a mercury diffusion pump backed up with a Cenco Hypervac oil pump. Pressures lower than 10- mm. of Hg are read on a calibrated ionization gauge.

Jan 1, 1939